CN105140052A - Super-capacitor carbon electrode material preparation method based on taxodiaceae plant cones - Google Patents
Super-capacitor carbon electrode material preparation method based on taxodiaceae plant cones Download PDFInfo
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- CN105140052A CN105140052A CN201510664714.7A CN201510664714A CN105140052A CN 105140052 A CN105140052 A CN 105140052A CN 201510664714 A CN201510664714 A CN 201510664714A CN 105140052 A CN105140052 A CN 105140052A
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- electrode material
- activation
- carbon electrode
- presoma
- carbon material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a super-capacitor carbon electrode material preparation method based on taxodiaceae plant cones. Dry fir cones act as the carbon source of porous activated carbon material. The precursor of porous carbon is acquired through pre-carbonization firstly, and then alkali metal hydroxide acts as a pore-forming agent to chemically activate the precursor through high temperature to acquire porous carbon material. The obtained porous carbon material has high specific surface area (989-1831m2g-1) and relatively large pore volume size (0.47-0.92m3g-1) and has a hierarchical porous structure. Excellent electrochemical capacitance performance is presented by the electrode prepared by the carbon material acting as active substance, e.g. the specific capacitance value is 255Fg-1 under current density of 10Ag-1 in 1.0MH2SO4 electrolyte. The renewable biological resource of fir cones with wide sources is fully utilized, the preparation technology is simple and low in cost and environment-friendly, and the obtained porous carbon material has huge application potential in the field of super-capacitor energy storage.
Description
Technical field
The present invention relates to a kind of porous carbon materials preparation and as the application of electrode material in ultracapacitor field, be specifically related to a kind of with metasequoia tree cone for raw material can be used for the preparation method of the porous carbon materials of ultracapacitor by pre-carbonization and high-temperature activation preparation.
Background technology
Ultracapacitor is a kind of Novel energy storage apparatus between conventional electrostatic capacitor and secondary rechargeable battery, and it has higher energy density relative to traditional capacitor, has higher power density relative to secondary cell.Because it has fast charging and discharging, serviceability temperature wide ranges, the advantage such as cycle life of pollution-free and overlength, have a wide range of applications in fields such as electronics, communication, Aero-Space and new energy electric motor vehicles, development prospect is wide.
Double electric layer capacitor based on material with carbon element is the focus of ultracapacitor research always, and the preparation of the carbon electrode material that cost performance is high is then the key of exploitation high-energy-density double electric layer capacitor.Due to high-specific surface area, high porosity, hierarchical porous structure, stable physicochemical property and cheap preparation cost, porous active material with carbon element enjoys favor in ultracapacitor market always.The preparation of porous carbon materials is primary raw material with biological material always, and exploration is easy to get, biomass source that is cheap, environmental protection has the porous carbon materials of high electrochemical capacitive property in order to preparation, is the important directions of super capacitor carbon electrode material research.
The taxodiaceae plant comprising metasequoia is in China and have very wide growth distribution area in the world, and only China's building material industry is derived from Chinese fir with regard to there being the timber more than 1/4th.The cone that Chinese fir output quantities countless is every year huge, because it is without special purpose, seldom causes the concern of people.If utilize this aboundresources of Chinese fir cone to be easy to get, free of contamination biomass resource is carbon source, and research preparation can have the electrode material for super capacitor of high specific capacitance value, or for other field, will bring good economic benefit and environmental benefit undoubtedly.Take biological material as carbon source, through preliminary carbonization with to activate further or carbonization and activation are synchronously carried out being prepare the conventional method of porous carbon materials two kinds, and chemical activation especially using highly basic (as potassium hydroxide) as activator time, then have more the unique advantages such as activation is efficient, technique is simple, pollution-free, be thus widely used in the preparation of porous active material with carbon element.
And up to now, also do not have with taxodiaceae plant cone for the pertinent literature and patent report that can be used for ultracapacitor porous carbon electrode material prepared by raw material.
Summary of the invention
The object of the present invention is to provide a kind of with the metasequoia of drying tree cone for raw material preparation has the method for the porous carbon electrode material of excellent electrochemical capacitive property, to solve the problem that on market, normal activated carbon ratio capacitance value is lower, and then promote the research and development of high performance-price ratio, high-energy-density electric double layer electricity super capacitor device.
For solving the problem, the present invention specifically by the following technical solutions:
Prepare a method for super capacitor carbon electrode material based on taxodiaceae plant cone, comprise the steps:
(1), by Chinese fir cone drying, pulverize and be placed in pyrolysis furnace, with 2 ~ 10 DEG C of min in one or more mixed atmospheres in nitrogen, helium, argon gas
-1heating rate be warming up to 300 ~ 500 DEG C and keep 0.5 ~ 5h to carry out preliminary carbonization to raw material, naturally cooling after must activate presoma;
(2), by step (one) gained activation presoma and NaOH or potassium hydroxide or its mixture press the quality of 1:1 ~ 1:5 than Homogeneous phase mixing, in tube furnace with one or more mists in nitrogen, helium, argon gas for protective gas is with 2 ~ 10 DEG C of min
-1heating rate be warming up to 600 ~ 800 DEG C and keep 0.5 ~ 5h to carry out high temeperature chemistry activation and pore to step (one) gained activation presoma, naturally must activation products after cooling;
(3), by the activation products of step (two) gained first carry out neutralisation treatment with one or more in hydrochloric acid, sulfuric acid, nitric acid, then by washed with de-ionized water to neutral, after super-dry process, obtain metasequoia tree hole, cone Quito active carbon material;
(4), with step (three) gained porous carbon materials for active material, with polytetrafluoroethylene aqueous emulsion for binding agent, being conductive agent with acetylene black, take nickel foam as collector electrode, preparation work electrode.Using platinum plate electrode and saturated calomel electrode electrode as to electrode and reference electrode, with the aqueous solution of certain density acid or alkali for electrolyte carries out electrochemical capacitor performance test to gained porous carbon materials.
Beneficial effect of the present invention:
1, Taxodiaceae (metasequoia) cone is for make for preparing porous active material with carbon element as raw material first, and aboundresources is easy to get, and what make extensive preparation becomes possibility, twice laid, embodies good economy and environment benefit;
2, after activation, gained material with carbon element has high-specific surface area, larger pore volume volume and hierarchical porous structure, architecture basics has been established in this realization being double electric layer capacitor high specific capacitance value, in addition the nitrogen of high level and the existence of oxygen element, on the one hand can intensifier electrode material wettability in the electrolytic solution, also extra fake capacitance can be provided, to promote the raising of carbon electrode material ratio capacitance value further on the other hand;
3, present invention process is simple, efficient, and prepared metasequoia tree cone Quito mesoporous activated carbon electrode is at 6.0MKOH and 1.0MH
2sO
4in aqueous electrolyte, ratio capacitance value reaches as high as 326Fg respectively
-1and 341Fg
-1there is good multiplying power and stable cycle life, show excellent electrochemical capacitor performance, it is a kind of double electric layer electrochemical capacitors carbon electrode material compared with high performance-price ratio, this material is also expected at battery electrode material simultaneously, gas, liquid adsorbs, and the field such as catalyst and catalyst carrier is applied.
Accompanying drawing explanation
Fig. 1 is scanning electron microscopy (SEM) photo of embodiment 3 gained porous charcoal.
Fig. 2 is transmission electron microscope (TEM) photo of embodiment 3 gained porous charcoal.
Fig. 3 is the nitrogen adsorption desorption curve of embodiment 4 gained porous charcoal.
Fig. 4 be the current density of embodiment 2, embodiment 3 and embodiment 4 gained porous carbon electrode material with quality than capacitance relation curve.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.The following example only for illustration of the present invention, but is not used for limiting practical range of the present invention.
embodiment 1
By the metasequoia cone of drying, pulverize and be placed in pyrolysis furnace, with 10 DEG C of min in nitrogen atmosphere
-1heating rate be warming up to 400 DEG C and keep 2h, naturally cooling after must activate presoma; By the presoma of gained with NaOH with the quality of 1:1 than Homogeneous phase mixing, take nitrogen as protective gas, with 10 DEG C of min in tube furnace
-1be warming up to the further activation processing of 800 DEG C for heating rate and keep 2h, naturally obtaining activation products after cooling; By the activation products of gained with after nitric acid neutralisation treatment, then spend Ion Cleaning to neutral, after 80 DEG C of dry process, namely obtain metasequoia cone porous carbon materials, porous carbon materials specific area prepared under this condition is 1057m
2g
-1, pore volume is 0.53m
3g
-1.
Get porous charcoal prepared by 3mg as active material, by active material: acetylene black: the quality of polytetrafluoroethylene=85:10:5 compares Homogeneous phase mixing, with the pressure of 15MPa by mixed slurry compacting on nickel foam collector, make ultracapacitor single electrode, and at 1.0MH
2sO
4electrolyte in carry out the electro-chemical test of single work electrode.Wherein foam nickel electrode, saturated calomel electrode and platinum plate electrode are respectively as work electrode, reference electrode and to electrode.Electro-chemical test shows, at 0.5Ag
-1current density under be 274Fg than its electric capacity
-1.
embodiment 2
By the metasequoia cone of drying, pulverize and be placed in pyrolysis furnace, with 4 DEG C of min in nitrogen atmosphere
-1heating rate be warming up to 500 DEG C and keep 1h, naturally cooling after must activate presoma; By the presoma of gained with potassium hydroxide with the quality of 1:3 than Homogeneous phase mixing, take nitrogen as protective gas, with 4 DEG C of min in tube furnace
-1be warming up to the further activation processing of 600 DEG C for heating rate and keep 1h, naturally obtaining activation products after cooling; By the activation products of gained with after hydrochloric acid neutralisation treatment, then spend Ion Cleaning to neutral, after 80 DEG C of dry process, namely obtain porous carbon materials, porous carbon materials specific area prepared under this condition is 1145m
2g
-1, pore volume is 0.57m
3g
-1.
The preparation of work electrode is identical with embodiment 1 with electrochemical test method.Electro-chemical test shows, when current density is 0.5Ag
-1and 5Ag
-1, time its ratio capacitance value be respectively 298Fg
-1and 229Fg
-1.(accompanying drawing 4A)
embodiment 3
The preparation method of porous carbon materials becomes except 700 DEG C from 600 DEG C except activation temperature, and other parameters are identical with embodiment 2.Scanning electron microscopy (SEM) photo of this embodiment gained material with carbon element is as shown in accompanying drawing 1 and Figure of abstract, transmission electron microscope (TEM) photo as shown in Figure 2, resulting materials shows three-dimensional porous property and amorphism structure, and its nitrogen adsorption desorption curve (accompanying drawing 3) shows that its specific area reaches 1831m
2g
-1, pore volume is 0.92m
3g
-1.
The preparation of work electrode is identical with embodiment 1 with electrochemical test method.Electro-chemical test shows, in 6.0MKOH electrolyte, when current density is 0.5Ag
-1and 10Ag
-1, time its ratio capacitance value be respectively 326Fg
-1and 237Fg
-1, at 1.0MH
2sO
4electrolyte, most high specific capacitance value can reach 341Fg
-1(accompanying drawing 4B)
embodiment 4
The preparation method of porous carbon materials becomes except 800 DEG C from 600 DEG C except activation temperature, and other parameters are identical with embodiment 2.This embodiment gained material with carbon element specific area reaches 1625m
2g
-1, pore volume is 0.81m
3g
-1.
The preparation of work electrode is identical with embodiment 1 with electrochemical test method.Electro-chemical test shows, in 6.0MKOH electrolyte, when current density is 1Ag
-1and 10Ag
-1, time its ratio capacitance value be respectively 226Fg
-1and 189Fg
-1(accompanying drawing 4C).
embodiment 5
By the metasequoia cone of drying, pulverize and be placed in pyrolysis furnace, with 2 DEG C of min in argon gas atmosphere
-1heating rate be warming up to 300 DEG C and keep 5h, naturally cooling after must activate presoma; By the presoma of gained with NaOH with the quality of 1:5 than Homogeneous phase mixing, take argon gas as protective gas, with 2 DEG C of min in tube furnace
-1be warming up to the further activation processing of 550 DEG C for heating rate and keep 5h, naturally obtaining activation products after cooling; By the activation products of gained with after nitric acid neutralisation treatment, then spend Ion Cleaning to neutral, after 80 DEG C of dry process, namely obtain metasequoia cone porous carbon materials, porous carbon materials specific area prepared under this condition is 989m
2g
-1, pore volume is 0.47m
3g
-1.
The preparation of work electrode is identical with embodiment 1 with electrochemical test method.Electro-chemical test shows, when current density is 0.5Ag
-1time, its ratio capacitance value is 251Fg
-1.
Claims (4)
1. prepare a method for super capacitor carbon electrode material based on taxodiaceae plant cone, it is characterized in that, comprise the steps:
(1), by Chinese fir cone drying, pulverize and be placed in pyrolysis furnace, in inert gas atmosphere, carry out pre-carbonization treatment, naturally must activate presoma after cooling;
(2), by step (one) gained activation presoma and alkali metal hydroxide Homogeneous phase mixing, be that protective gas carries out chemical activation process to presoma with inert gas in tube furnace, naturally obtain activation products after cooling;
(3), by step (two) gained activation products first carry out neutralisation treatment with acid, then by washed with de-ionized water to neutral, after drying process, namely obtain hole, Chinese fir cone Quito active carbon material.
2. a kind of method preparing super capacitor carbon electrode material based on taxodiaceae plant cone according to claim 1, it is characterized in that, inert gas described in step () is one or more mixing in nitrogen, argon gas, helium, pre-carburizing temperature is 300 ~ 500 DEG C and keeps 0.5 ~ 5h, and wherein heating rate is 2 ~ 10 DEG C of min
-1.
3. a kind of method preparing super capacitor carbon electrode material based on taxodiaceae plant cone according to claim 1, it is characterized in that, inert gas described in step (two) is one or more mixing in nitrogen, argon gas, helium, the activation presoma of step (two) gained and alkali metal hydroxide mass ratio are 1:1 ~ 1:5, activation temperature is 600 ~ 800 DEG C and keeps 0.5 ~ 5h, and wherein heating rate is 2 ~ 10 DEG C of min
-1.
4. a kind of method preparing super capacitor carbon electrode material based on taxodiaceae plant cone according to claim 1, it is characterized in that, alkali metal hydroxide described in step (two) is NaOH or potassium hydroxide or the two mixture, and the acid described in step (three) is one or more in hydrochloric acid, sulfuric acid, nitric acid.
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| CN106430187A (en) * | 2016-09-20 | 2017-02-22 | 湖南南方搏云新材料股份有限公司 | Method of using uncured carbon felt leftover material for preparing supercapacitor electrode activated carbon |
| CN106803595A (en) * | 2016-12-28 | 2017-06-06 | 深圳大学 | A kind of carbon-based oxygen reduction catalyst and preparation method and application |
| CN109473295A (en) * | 2017-09-07 | 2019-03-15 | 北京化工大学 | A method of electrode of super capacitor carbon material is prepared using apple |
| CN111785535A (en) * | 2020-08-04 | 2020-10-16 | 山东理工大学 | Preparation method of self-activated high-specific-capacitance carbon nanotube electrode |
| WO2021036548A1 (en) * | 2019-08-26 | 2021-03-04 | 山东大学 | Method for ultrasonic-assisted preparation of super active carbon and application thereof |
| CN114758900A (en) * | 2022-04-27 | 2022-07-15 | 深圳大学 | Biomass porous carbon material, preparation method thereof and supercapacitor |
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| CN106430187A (en) * | 2016-09-20 | 2017-02-22 | 湖南南方搏云新材料股份有限公司 | Method of using uncured carbon felt leftover material for preparing supercapacitor electrode activated carbon |
| CN106803595A (en) * | 2016-12-28 | 2017-06-06 | 深圳大学 | A kind of carbon-based oxygen reduction catalyst and preparation method and application |
| WO2018121365A1 (en) * | 2016-12-28 | 2018-07-05 | 深圳大学 | Carbon-based oxygen reduction catalyst, preparation method therefor and use thereof |
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| WO2021036548A1 (en) * | 2019-08-26 | 2021-03-04 | 山东大学 | Method for ultrasonic-assisted preparation of super active carbon and application thereof |
| CN111785535A (en) * | 2020-08-04 | 2020-10-16 | 山东理工大学 | Preparation method of self-activated high-specific-capacitance carbon nanotube electrode |
| CN111785535B (en) * | 2020-08-04 | 2022-03-11 | 山东理工大学 | Preparation method of self-activated high-specific-capacitance carbon nanotube electrode |
| CN114758900A (en) * | 2022-04-27 | 2022-07-15 | 深圳大学 | Biomass porous carbon material, preparation method thereof and supercapacitor |
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